A series of AAl(12)O(19) (A=La, Sr, Ba, Ca, Ce), AMAl(11)O(19) (A=La, Sr; M=Cu, Mn, Fe, Ni, Mg) and Sr1-xLaxMnAl11O19 (x=0.2-0.8) hexaaluminates were prepared successfully using urea combustion method. The influences of the molar ratio (R) of urea to the total metal ions in hexaaluminates and the urea combustion temperature on the formation of the hexaaluminates were investigated. The structure of the hexaaluminates was characterized using X-ray powder diffraction (XRD) and temperature-programmed reduction (TPR). The catalytic activity for methane combustion was evaluated. The results indicated that the preparation conditions were: for LaAl12O19, the value of R was 3, the combustion time was in the range from 40 to 60min, and the combustion temperature was not less than 500 degrees C; For LaFeAl11O19 and LaMnAl11O19, the value of R was 3-7, the combustion time was 40min, and the combustion temperature was less than 500 and 400 degrees C, respectively; for AAl(12)O(19) (A=Sr, Ba, Ca, Ce), LaMAl11O19 (M=Cu, Ni, Mg), SrMAl11O19 (M=Cu, Mn, Fe, Ni, Mg) and Sr1-xLaxMnAl11O19 (x=0.2-0.8), the value of R was 3, the combustion time was 40min, and the combustion temperature was 500 degrees C. The prepared hexaaluminates had pure hexaaluminate phase structure and excellent catalytic activity in the methane combustion. (C) 2008 Elsevier B.V. All rights reserved.